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Hydrochloric Acid → 4-(4-Fluoro-2-(tetrahydro-2H-pyran-4-yloxy)phenylamino)-5-methylthieno[2,3-d]pyrimidine-6-carboxylic acid

HRID 450534
ノート
印刷プレビュー

反応式

HRID 450534 の反応式
[F:1][C:2]1[CH:7]=[CH:6][C:5]([NH:8][C:9]2[C:10]3[C:17]([CH3:18])=[C:16]([C:19]([O:21]C)=[O:20])[S:15][C:11]=3[N:12]=[CH:13][N:14]=2)=[C:4]([O:23][CH:24]2[CH2:29][CH2:28][O:27][CH2:26][CH2:25]2)[CH:3]=1.O.[OH-].[Li+].Cl>C1COCC1.O>[F:1][C:2]1[CH:7]=[CH:6][C:5]([NH:8][C:9]2[C:10]3[C:17]([CH3:18])=[C:16]([C:19]([OH:21])=[O:20])[S:15][C:11]=3[N:12]=[CH:13][N:14]=2)=[C:4]([O:23][CH:24]2[CH2:25][CH2:26][O:27][CH2:28][CH2:29]2)[CH:3]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 168937Lithium hydroxide, monohydrateHCID 461820444-[4-Fluoro-2-(tetrahydro-pyran-4-yloxy)-phenylamino]-5-methyl-thieno[2,3-d]pyrimidine-6-carboxylic acid methylester

生成物 1

HCID 461826634-(4-Fluoro-2-(tetrahydro-2H-pyran-4-yloxy)phenylamino)-5-methylthieno[2,3-d]pyrimidine-6-carboxylic acid収率 99.2%

試薬・触媒・溶媒 1

HCID 21881883
Oxolane--water (1/1)
溶媒

実験手順

Methyl 4-(4-fluoro-2-(tetrahydro-2H-pyran-4-yloxy)phenylamino)-5-methylthieno[2,3-d]pyrimidine-6-carboxylate (9.0 g, 21.6 mmol) was suspended in THF/water (1:1; 200 mL). Into this solution was added lithium hydroxide monohydrate (5.31 g, 126.5 mmol) and the reaction stirred at ambient temperature overnight. The solution was cooled in an ice-bath and concentrated hydrochloric acid added until the solution reached pH 4. The precipitate was collected, washed with water and dried over P2O5 to yield off-white solid (8.642 g, 99%).

後処理

  1. temperatureThe solution was cooled in an ice-bath
  2. customThe precipitate was collected
  3. washwashed with water
  4. dry with materialdried over P2O5

出典と根拠

ORDレコード
ord-47c28839f1634a4780bb1c8c2e35f14e
出典データセット
uspto-grants-2013_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08486953B2

反応ノート

読み込み中…

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